Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Elena A. Vinogradova' 'Olga Yu. Vassilyeva' 'Volodymyr N. Kokozay' 'Brian W. Skelton' 'Jens K. Bjernemose' 'Paul R. Raithby' _publ_contact_author_name 'Prof Paul Raithby' _publ_contact_author_address ; Prof Paul Raithby Department of Chemistry University of Bath Claverton Down Bath Avon BA2 7AY UNITED KINGDOM ; _publ_contact_author_email 'P.R.RAITHBY@BATH.AC.UK' _publ_section_title ; Novel heterometallic Cd/Cu complexes prepared using zerovalent copper: control of the nuclearity and structural diversity by halide counterions ; _publ_section_references ; Sheldrick, G M. (1996). SADABS. Program for Empirical Absorption Correction of Area Detector Data. University of Gottingen, Germany. Siemens (1995). SMART and SAINT. Area-Detector Control and Integration Software. Siemens Analytical X-ray Systems Inc., Madison, Wisconsin, USA. Hall, S.R., King, G.S.D., and Stewart., J.M. (1995). The Xtal 3.5 User's Manual. University of Western Australia, Lamb: Perth. ; data_h01prr35 _database_code_CSD 178072 _audit_creation_method SHELXL-97 _chemical_name_systematic ; COMPLEX 1 ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H52 Cd2 Cu2 I4 N4 O6 S2' _chemical_formula_sum 'C20 H52 Cd2 Cu2 I4 N4 O6 S2' _chemical_formula_weight 1368.32 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cd' 'Cd' -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.4240(3) _cell_length_b 18.1880(7) _cell_length_c 13.4520(5) _cell_angle_alpha 90.00 _cell_angle_beta 97.576(2) _cell_angle_gamma 90.00 _cell_volume 2043.07(13) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 19145 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.224 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1292 _exptl_absorpt_coefficient_mu 5.212 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.3803 _exptl_absorpt_correction_T_max 0.5086 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method '309 2.0 degree images' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35254 _diffrn_reflns_av_R_equivalents 0.0837 _diffrn_reflns_av_sigmaI/netI 0.0624 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 27.47 _reflns_number_total 4670 _reflns_number_gt 3160 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinski & Minor, 1997)' _computing_data_reduction 'HKL Denzo & Scalepack (Otwinski & Minor 1997)' _computing_structure_solution 'DirDif-99 (Beurskens, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w=3D1/[\s^2^(Fo^2^)+(0.0462P)^2^+2.1698P] where = P=3D(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4670 _refine_ls_number_parameters 209 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0800 _refine_ls_R_factor_gt 0.0412 _refine_ls_wR_factor_ref 0.0977 _refine_ls_wR_factor_gt 0.0877 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C12 C 0.7413(8) 0.9256(4) 0.4776(5) 0.0472(18) Uani 1 1 d . A . H12A H 0.7860 0.8777 0.4599 0.057 Uiso 1 1 calc R . . H12B H 0.6495 0.9376 0.4264 0.057 Uiso 1 1 calc R . . C13 C 0.6869(10) 0.9208(5) 0.5784(6) 0.068(3) Uani 1 1 d . A . H13A H 0.6156 0.9628 0.5877 0.082 Uiso 1 1 calc R . . H13B H 0.6252 0.8749 0.5831 0.082 Uiso 1 1 calc R . . C141 C 0.7684(12) 0.9406(6) 0.7525(6) 0.090(4) Uani 1 1 d . A . H14A H 0.7192 0.9894 0.7469 0.136 Uiso 1 1 calc R . . H14B H 0.8585 0.9407 0.8066 0.136 Uiso 1 1 calc R . . H14C H 0.6889 0.9042 0.7674 0.136 Uiso 1 1 calc R . . C142 C 0.8989(12) 0.8494(5) 0.6665(10) 0.106(4) Uani 1 1 d . A . H14D H 0.9366 0.8366 0.6028 0.159 Uiso 1 1 calc R . . H14E H 0.8198 0.8131 0.6819 0.159 Uiso 1 1 calc R . . H14F H 0.9897 0.8496 0.7202 0.159 Uiso 1 1 calc R . . C22 C 1.2524(8) 0.9881(4) 0.7654(5) 0.054(2) Uani 0.65 1 d P A 1 H22A H 1.2992 0.9684 0.7071 0.065 Uiso 0.65 1 calc PR A 1 H22B H 1.2390 0.9469 0.8116 0.065 Uiso 0.65 1 calc PR A 1 C23 C 1.3685(12) 1.0482(6) 0.8212(8) 0.043(3) Uani 0.65 1 d P A 1 H23A H 1.4653 1.0238 0.8561 0.051 Uiso 0.65 1 calc PR A 1 H23B H 1.4029 1.0828 0.7713 0.051 Uiso 0.65 1 calc PR A 1 C241 C 1.390(2) 1.1430(9) 0.9470(13) 0.065(5) Uani 0.65 1 d P A 1 H24A H 1.3266 1.1669 0.9938 0.098 Uiso 0.65 1 calc PR A 1 H24B H 1.4240 1.1798 0.9009 0.098 Uiso 0.65 1 calc PR A 1 H24C H 1.4848 1.1201 0.9846 0.098 Uiso 0.65 1 calc PR A 1 C242 C 1.2347(13) 1.0333(7) 0.9698(8) 0.050(3) Uani 0.65 1 d P A 1 H24D H 1.1817 1.0617 1.0178 0.075 Uiso 0.65 1 calc PR A 1 H24E H 1.3269 1.0072 1.0054 0.075 Uiso 0.65 1 calc PR A 1 H24F H 1.1591 0.9976 0.9357 0.075 Uiso 0.65 1 calc PR A 1 C22B C 1.2524(8) 0.9881(4) 0.7654(5) 0.054(2) Uani 0.35 1 d P A 2 H22C H 1.3369 1.0093 0.7294 0.065 Uiso 0.35 1 calc PR A 2 H22D H 1.2489 0.9342 0.7551 0.065 Uiso 0.35 1 calc PR A 2 C23B C 1.282(2) 1.0078(9) 0.8808(15) 0.044(5) Uani 0.35 1 d P A 2 H23C H 1.1932 0.9892 0.9148 0.053 Uiso 0.35 1 calc PR A 2 H23D H 1.3831 0.9848 0.9125 0.053 Uiso 0.35 1 calc PR A 2 C41B C 1.441(2) 1.1118(12) 0.8232(17) 0.052(6) Uani 0.35 1 d P A 2 H41A H 1.4226 1.0888 0.7568 0.078 Uiso 0.35 1 calc PR A 2 H41B H 1.5441 1.0956 0.8584 0.078 Uiso 0.35 1 calc PR A 2 H41C H 1.4409 1.1654 0.8158 0.078 Uiso 0.35 1 calc PR A 2 C42B C 1.331(4) 1.116(2) 0.982(3) 0.070(10) Uani 0.35 1 d P A 2 H42A H 1.3360 1.1700 0.9758 0.105 Uiso 0.35 1 calc PR A 2 H42B H 1.4359 1.0977 1.0115 0.105 Uiso 0.35 1 calc PR A 2 H42C H 1.2499 1.1029 1.0240 0.105 Uiso 0.35 1 calc PR A 2 C321 C 0.6518(10) 1.2134(4) 0.6501(6) 0.058(2) Uani 1 1 d . . . H32A H 0.6143 1.2028 0.7146 0.087 Uiso 1 1 calc R . . H32B H 0.5687 1.2403 0.6070 0.087 Uiso 1 1 calc R . . H32C H 0.7494 1.2432 0.6614 0.087 Uiso 1 1 calc R . . C322 C 0.7527(11) 1.1658(4) 0.4807(5) 0.060(2) Uani 1 1 d . . . H32D H 0.7806 1.1253 0.4381 0.091 Uiso 1 1 calc R . . H32E H 0.8461 1.1977 0.4975 0.091 Uiso 1 1 calc R . . H32F H 0.6646 1.1943 0.4446 0.091 Uiso 1 1 calc R . . Cu1 Cu 0.98135(9) 0.99592(4) 0.60848(5) 0.02817(18) Uani 1 1 d . . . Cd1 Cd 1.05654(5) 1.13226(2) 0.78967(3) 0.02717(13) Uani 1 1 d . A . I1 I 1.15415(6) 1.25620(2) 0.69633(3) 0.04458(15) Uani 1 1 d . . . I2 I 0.87040(5) 1.16118(3) 0.93737(3) 0.04459(15) Uani 1 1 d . . . O21 O 1.1000(5) 1.0209(2) 0.7323(3) 0.0333(10) Uani 1 1 d . . . O31 O 0.8429(5) 1.0999(2) 0.6516(3) 0.0382(11) Uani 1 1 d . . . N14 N 0.8259(6) 0.9217(3) 0.6585(4) 0.0383(13) Uani 1 1 d . . . N24 N 1.2932(6) 1.0869(3) 0.8899(4) 0.0381(13) Uani 1 1 d . . . S32 S 0.6933(2) 1.12998(10) 0.59145(13) 0.0417(4) Uani 1 1 d . A . O11 O 0.8592(5) 0.9807(2) 0.4797(3) 0.0330(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C12 0.040(4) 0.057(5) 0.045(4) -0.015(4) 0.009(3) -0.023(4) C13 0.061(5) 0.090(7) 0.053(5) -0.001(5) 0.004(4) -0.036(5) C141 0.116(8) 0.107(8) 0.057(5) -0.020(5) 0.048(6) -0.062(7) C142 0.079(7) 0.055(6) 0.190(13) 0.056(7) 0.042(8) -0.004(5) C22 0.048(4) 0.054(5) 0.052(5) -0.023(4) -0.027(4) 0.030(4) C23 0.029(6) 0.052(7) 0.045(6) 0.002(6) 0.000(5) 0.012(5) C241 0.054(11) 0.056(11) 0.078(13) -0.044(9) -0.020(8) 0.008(8) C242 0.038(6) 0.079(9) 0.032(6) 0.018(6) 0.005(5) 0.007(6) C22B 0.048(4) 0.054(5) 0.052(5) -0.023(4) -0.027(4) 0.030(4) C23B 0.030(10) 0.029(10) 0.062(14) 0.011(10) -0.035(10) 0.002(8) C41B 0.023(11) 0.060(15) 0.067(14) -0.010(11) -0.014(9) 0.025(10) C42B 0.05(2) 0.08(3) 0.07(2) -0.004(17) -0.020(15) 0.000(16) C321 0.063(5) 0.059(5) 0.050(5) -0.001(4) 0.001(4) 0.028(4) C322 0.089(6) 0.047(5) 0.047(5) 0.013(4) 0.012(4) 0.026(4) Cu1 0.0301(4) 0.0284(4) 0.0252(4) -0.0027(3) 0.0009(3) -0.0016(3) Cd1 0.0288(3) 0.0270(2) 0.0247(2) -0.00063(18) 0.00013(18) 0.00265(19) I1 0.0573(3) 0.0357(3) 0.0400(3) 0.0073(2) 0.0035(2) -0.0098(2) I2 0.0417(3) 0.0551(3) 0.0392(3) -0.0049(2) 0.0139(2) 0.0032(2) O21 0.033(2) 0.033(2) 0.031(2) -0.0039(19) -0.0069(18) 0.0141(19) O31 0.036(2) 0.034(3) 0.040(3) -0.012(2) -0.013(2) 0.012(2) N14 0.046(3) 0.034(3) 0.035(3) 0.004(2) 0.008(3) -0.007(3) N24 0.037(3) 0.040(3) 0.032(3) -0.004(3) -0.014(2) 0.003(3) S32 0.0367(10) 0.0422(10) 0.0433(10) 0.0011(8) -0.0057(7) 0.0044(8) O11 0.028(2) 0.044(3) 0.026(2) -0.0058(19) 0.0037(18) -0.010(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are = taken into account individually in the estimation of esds in distances, = angles and torsion angles; correlations between esds in cell parameters are = only used when they are defined by crystal symmetry. An approximate = (isotropic) treatment of cell esds is used for estimating esds involving l.s. = planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C12 O11 1.409(7) . ? C12 C13 1.490(9) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 N14 1.482(9) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C141 N14 1.453(9) . ? C141 H14A 0.9800 . ? C141 H14B 0.9800 . ? C141 H14C 0.9800 . ? C142 N14 1.450(10) . ? C142 H14D 0.9800 . ? C142 H14E 0.9800 . ? C142 H14F 0.9800 . ? C22 O21 1.432(7) . ? C22 C23 1.588(13) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 N24 1.380(11) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C241 N24 1.461(15) . ? C241 H24A 0.9800 . ? C241 H24B 0.9800 . ? C241 H24C 0.9800 . ? C242 N24 1.577(11) . ? C242 H24D 0.9800 . ? C242 H24E 0.9800 . ? C242 H24F 0.9800 . ? C23B N24 1.444(18) . ? C23B H23C 0.9900 . ? C23B H23D 0.9900 . ? C41B N24 1.69(2) . ? C41B H41A 0.9800 . ? C41B H41B 0.9800 . ? C41B H41C 0.9800 . ? C42B N24 1.34(3) . ? C42B H42A 0.9800 . ? C42B H42B 0.9800 . ? C42B H42C 0.9800 . ? C321 S32 1.766(7) . ? C321 H32A 0.9800 . ? C321 H32B 0.9800 . ? C321 H32C 0.9800 . ? C322 S32 1.758(7) . ? C322 H32D 0.9800 . ? C322 H32E 0.9800 . ? C322 H32F 0.9800 . ? Cu1 O21 1.881(4) . ? Cu1 O11 1.915(4) . ? Cu1 O11 1.952(4) 3_776 ? Cu1 N14 2.055(5) . ? Cu1 O31 2.335(4) . ? Cu1 Cu1 2.9799(14) 3_776 ? Cd1 O21 2.216(4) . ? Cd1 N24 2.401(5) . ? Cd1 O31 2.481(4) . ? Cd1 I2 2.7395(6) . ? Cd1 I1 2.7580(6) . ? O31 S32 1.508(4) . ? O11 Cu1 1.952(4) 3_776 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O11 C12 C13 108.9(5) . . ? O11 C12 H12A 109.9 . . ? C13 C12 H12A 109.9 . . ? O11 C12 H12B 109.9 . . ? C13 C12 H12B 109.9 . . ? H12A C12 H12B 108.3 . . ? N14 C13 C12 110.7(6) . . ? N14 C13 H13A 109.5 . . ? C12 C13 H13A 109.5 . . ? N14 C13 H13B 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 108.1 . . ? N14 C141 H14A 109.5 . . ? N14 C141 H14B 109.5 . . ? H14A C141 H14B 109.5 . . ? N14 C141 H14C 109.5 . . ? H14A C141 H14C 109.5 . . ? H14B C141 H14C 109.5 . . ? N14 C142 H14D 109.5 . . ? N14 C142 H14E 109.5 . . ? H14D C142 H14E 109.5 . . ? N14 C142 H14F 109.5 . . ? H14D C142 H14F 109.5 . . ? H14E C142 H14F 109.5 . . ? O21 C22 C23 109.4(6) . . ? O21 C22 H22A 109.8 . . ? C23 C22 H22A 109.8 . . ? O21 C22 H22B 109.8 . . ? C23 C22 H22B 109.8 . . ? H22A C22 H22B 108.2 . . ? N24 C23 C22 111.0(8) . . ? N24 C23 H23A 109.4 . . ? C22 C23 H23A 109.4 . . ? N24 C23 H23B 109.4 . . ? C22 C23 H23B 109.4 . . ? H23A C23 H23B 108.0 . . ? N24 C241 H24A 109.5 . . ? N24 C241 H24B 109.5 . . ? H24A C241 H24B 109.5 . . ? N24 C241 H24C 109.5 . . ? H24A C241 H24C 109.5 . . ? H24B C241 H24C 109.5 . . ? N24 C242 H24D 109.5 . . ? N24 C242 H24E 109.5 . . ? H24D C242 H24E 109.5 . . ? N24 C242 H24F 109.5 . . ? H24D C242 H24F 109.5 . . ? H24E C242 H24F 109.5 . . ? N24 C23B H23C 110.1 . . ? N24 C23B H23D 110.1 . . ? H23C C23B H23D 108.4 . . ? N24 C41B H41A 109.5 . . ? N24 C41B H41B 109.5 . . ? H41A C41B H41B 109.5 . . ? N24 C41B H41C 109.5 . . ? H41A C41B H41C 109.5 . . ? H41B C41B H41C 109.5 . . ? N24 C42B H42A 109.5 . . ? N24 C42B H42B 109.5 . . ? H42A C42B H42B 109.5 . . ? N24 C42B H42C 109.5 . . ? H42A C42B H42C 109.5 . . ? H42B C42B H42C 109.5 . . ? S32 C321 H32A 109.5 . . ? S32 C321 H32B 109.5 . . ? H32A C321 H32B 109.5 . . ? S32 C321 H32C 109.5 . . ? H32A C321 H32C 109.5 . . ? H32B C321 H32C 109.5 . . ? S32 C322 H32D 109.5 . . ? S32 C322 H32E 109.5 . . ? H32D C322 H32E 109.5 . . ? S32 C322 H32F 109.5 . . ? H32D C322 H32F 109.5 . . ? H32E C322 H32F 109.5 . . ? O21 Cu1 O11 174.36(18) . . ? O21 Cu1 O11 99.04(17) . 3_776 ? O11 Cu1 O11 79.20(18) . 3_776 ? O21 Cu1 N14 99.0(2) . . ? O11 Cu1 N14 84.93(19) . . ? O11 Cu1 N14 149.49(19) 3_776 . ? O21 Cu1 O31 79.00(15) . . ? O11 Cu1 O31 96.65(16) . . ? O11 Cu1 O31 112.37(17) 3_776 . ? N14 Cu1 O31 95.14(19) . . ? O21 Cu1 Cu1 137.94(14) . 3_776 ? O11 Cu1 Cu1 40.05(11) . 3_776 ? O11 Cu1 Cu1 39.15(11) 3_776 3_776 ? N14 Cu1 Cu1 120.50(15) . 3_776 ? O31 Cu1 Cu1 108.88(11) . 3_776 ? O21 Cd1 N24 73.62(16) . . ? O21 Cd1 O31 70.07(13) . . ? N24 Cd1 O31 143.66(15) . . ? O21 Cd1 I2 124.41(11) . . ? N24 Cd1 I2 99.85(13) . . ? O31 Cd1 I2 99.22(10) . . ? O21 Cd1 I1 121.05(11) . . ? N24 Cd1 I1 105.16(13) . . ? O31 Cd1 I1 94.79(11) . . ? I2 Cd1 I1 114.00(2) . . ? C22 O21 Cu1 121.7(4) . . ? C22 O21 Cd1 117.0(4) . . ? Cu1 O21 Cd1 115.85(18) . . ? S32 O31 Cu1 124.7(2) . . ? S32 O31 Cd1 142.0(2) . . ? Cu1 O31 Cd1 92.37(13) . . ? C142 N14 C141 109.6(7) . . ? C142 N14 C13 109.3(7) . . ? C141 N14 C13 108.3(7) . . ? C142 N14 Cu1 109.7(5) . . ? C141 N14 Cu1 115.5(5) . . ? C13 N14 Cu1 104.2(4) . . ? C42B N24 C23 137.9(16) . . ? C42B N24 C23B 118.7(18) . . ? C23 N24 C23B 57.7(10) . . ? C42B N24 C241 35.8(13) . . ? C23 N24 C241 115.7(9) . . ? C23B N24 C241 139.9(11) . . ? C42B N24 C242 71.4(15) . . ? C23 N24 C242 110.8(8) . . ? C23B N24 C242 54.6(10) . . ? C241 N24 C242 106.1(9) . . ? C42B N24 C41B 106.0(15) . . ? C23 N24 C41B 49.1(8) . . ? C23B N24 C41B 105.3(12) . . ? C241 N24 C41B 72.1(10) . . ? C242 N24 C41B 147.8(8) . . ? C42B N24 Cd1 117.3(16) . . ? C23 N24 Cd1 102.7(5) . . ? C23B N24 Cd1 104.9(7) . . ? C241 N24 Cd1 114.8(8) . . ? C242 N24 Cd1 106.5(5) . . ? C41B N24 Cd1 102.9(7) . . ? O31 S32 C322 106.2(3) . . ? O31 S32 C321 105.8(3) . . ? C322 S32 C321 99.0(4) . . ? C12 O11 Cu1 114.5(4) . . ? C12 O11 Cu1 133.1(4) . 3_776 ? Cu1 O11 Cu1 100.80(17) . 3_776 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.419 _refine_diff_density_min -1.141 _refine_diff_density_rms 0.174 ####END #======================================================================= # Data block for single structure (one for each study in the paper) #======================================================================= data_lv579 _database_code_CSD 178073 _audit_creation_method Xtal3.6 _audit_creation_date 01-08-22 _audit_update_record ? # 2. EXPERIMENTAL DATA #--------------------- _chemical_name_systematic ; COMPLEX 2 ; # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C20 H52 Br6 Cd2 Cu3 N4 O6 S2' _chemical_formula_moiety ? _chemical_formula_weight 1403.67 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C_1_2/c_1 _symmetry_space_group_name_Hall -c_2yc loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,+y,1/2-z -x,-y,-z +x,-y,1/2+z 1/2+x,1/2+y,+z 1/2-x,1/2+y,1/2-z 1/2-x,1/2-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 31.395(2) _cell_length_b 8.0019(6) _cell_length_c 18.7480(10) _cell_angle_alpha 90.00000 _cell_angle_beta 118.1070(10) _cell_angle_gamma 90.00000 _cell_volume 4154.4(5) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 2.244 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 4848 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 20.1 _cell_measurement_temperature 150 _exptl_absorpt_coefficient_mu 8.425 _exptl_crystal_description plate _exptl_crystal_size_max .25 _exptl_crystal_size_mid .17 _exptl_crystal_size_min .05 _exptl_crystal_size_rad ? _exptl_crystal_colour dark_green _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .51 _exptl_absorpt_correction_T_max .86 _diffrn_reflns_number 30649 _reflns_number_total 5514 _reflns_Friedel_coverage 0 _reflns_number_gt 4002 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 28.99 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents .065 _diffrn_reflns_limit_h_min -42 _diffrn_reflns_limit_h_max 37 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 25 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .035 _refine_ls_wR_factor_ref .037 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_number_reflns 4002 _refine_ls_number_parameters 206 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .003 _refine_diff_density_min -1.265 _refine_diff_density_max 1.298 _refine_ls_extinction_method ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF SORTRF' _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 80 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 208 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' Br ? 0 24 -.374 2.456 'Int Tables Vol IV Tables 2.2B and 2.3.1' Cd ? 0 8 -1.005 1.202 'Int Tables Vol IV Tables 2.2B and 2.3.1' Cu ? 0 12 .263 1.266 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 16 .004 .003 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 24 .008 .006 'Int Tables Vol IV Tables 2.2B and 2.3.1' S ? 0 8 .11 .124 'Int Tables Vol IV Tables 2.2B and 2.3.1' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Cd1 .134096(13) .87778(4) .47934(2) .02306(16) Uani ? ? 1.00000 ? ? Br1 .212652(18) 1.04381(6) .56011(3) .0261(2) Uani ? ? 1.00000 ? ? Br2 .08577(2) .86364(7) .32212(3) .0347(3) Uani ? ? 1.00000 ? ? Br3 .10406(2) .71796(7) .56676(4) .0385(3) Uani ? ? 1.00000 ? ? Cu1 .25000 .75000 .50000 .0170(3) Uani ? ? 1.00000 ? ? Cu2 .16656(2) .66611(7) .34796(3) .0227(3) Uani ? ? 1.00000 ? ? O11 .21408(11) .8389(4) .39282(18) .0214(14) Uani ? ? 1.00000 ? ? C12 .22945(19) .9063(6) .3392(3) .029(2) Uani ? ? 1.00000 ? ? C13 .1865(2) .8972(6) .2553(3) .030(2) Uani ? ? 1.00000 ? ? N14 .16665(15) .7243(5) .2393(3) .031(2) Uani ? ? 1.00000 ? ? C141 .1990(2) .6127(7) .2241(3) .037(3) Uani ? ? 1.00000 ? ? C142 .1192(2) .7287(7) .1649(3) .041(3) Uani ? ? 1.00000 ? ? O21 .18453(11) .6522(4) .46418(18) .0206(14) Uani ? ? 1.00000 ? ? C22 .17648(18) .4858(6) .4832(3) .026(2) Uani ? ? 1.00000 ? ? C23 .13081(19) .4227(6) .4132(3) .029(2) Uani ? ? 1.00000 ? ? N24 .13327(15) .4370(5) .3358(3) .033(2) Uani ? ? 1.00000 ? ? C241 .1634(2) .2965(7) .3323(4) .041(3) Uani ? ? 1.00000 ? ? C242 .0841(2) .4176(8) .2679(4) .048(3) Uani ? ? 1.00000 ? ? O1 .08559(13) 1.1128(4) .4702(2) .0346(17) Uani ? ? 1.00000 ? ? S1 .03786(5) 1.12928(19) .46790(9) .0277(7) Uani ? ? .884(5) ? ? S1' .0350(5) 1.1674(16) .4098(8) .037(7) Uani ? ? .116(5) ? ? C101 -.0062(2) 1.0310(7) .3781(4) .041(3) Uani ? ? 1.00000 ? ? C102 .0197(2) 1.3396(7) .4401(4) .047(3) Uani ? ? 1.00000 ? ? H12a .23979 1.01883 .35360 .03900 Uiso ? ? 1.00000 ? ? H12b .25573 .84239 .34139 .03900 Uiso ? ? 1.00000 ? ? H13a .16198 .97365 .25135 .04000 Uiso ? ? 1.00000 ? ? H13b .19588 .92696 .21540 .04000 Uiso ? ? 1.00000 ? ? H141a .22965 .60875 .27027 .05500 Uiso ? ? 1.00000 ? ? H141b .20243 .65522 .17928 .05500 Uiso ? ? 1.00000 ? ? H141c .18562 .50361 .21112 .05500 Uiso ? ? 1.00000 ? ? H142a .09692 .79910 .17391 .06000 Uiso ? ? 1.00000 ? ? H142b .10513 .61884 .15257 .06000 Uiso ? ? 1.00000 ? ? H142c .12195 .77045 .12073 .06000 Uiso ? ? 1.00000 ? ? H22a .20230 .41385 .49126 .03200 Uiso ? ? 1.00000 ? ? H22b .17312 .48503 .53189 .03200 Uiso ? ? 1.00000 ? ? H23a .12419 .31064 .42145 .03600 Uiso ? ? 1.00000 ? ? H23b .10355 .49063 .40838 .03600 Uiso ? ? 1.00000 ? ? H241a .19568 .30763 .37602 .05800 Uiso ? ? 1.00000 ? ? H241b .16457 .30143 .28274 .05800 Uiso ? ? 1.00000 ? ? H241c .15037 .19408 .33711 .05800 Uiso ? ? 1.00000 ? ? H242a .06341 .50558 .26803 .07300 Uiso ? ? 1.00000 ? ? H242b .07025 .31329 .27149 .07300 Uiso ? ? 1.00000 ? ? H242c .08445 .42065 .21712 .07300 Uiso ? ? 1.00000 ? ? H101a -.00495 1.07284 .33182 .04800 Uiso ? ? .884(5) ? ? H101b -.03796 1.04875 .37175 .04800 Uiso ? ? .884(5) ? ? H101c -.00069 .91213 .38098 .04800 Uiso ? ? .884(5) ? ? H102a .01637 1.36195 .38622 .05800 Uiso ? ? .884(5) ? ? H102b .04206 1.41613 .47627 .05800 Uiso ? ? .884(5) ? ? H102c -.01150 1.35999 .43593 .05800 Uiso ? ? .884(5) ? ? H101'a -.01085 .99086 .42172 .04800 Uiso ? ? .116(5) ? ? H101'b .00177 .93739 .35442 .04800 Uiso ? ? .116(5) ? ? H101'c -.03597 1.07711 .33779 .04800 Uiso ? ? .116(5) ? ? H102'a .02341 1.32775 .49141 .05800 Uiso ? ? .116(5) ? ? H102'b -.01405 1.36490 .40245 .05800 Uiso ? ? .116(5) ? ? H102'c .03820 1.43257 .43705 .05800 Uiso ? ? .116(5) ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Cd1 .02201(18) .02341(18) .02176(17) .00003(14) .00866(14) .00168(14) Br1 .0234(3) .0245(2) .0273(3) -.0019(2) .0093(2) -.0025(2) Br2 .0277(3) .0475(3) .0228(3) .0102(2) .0068(2) .0017(2) Br3 .0455(4) .0343(3) .0490(3) -.0013(2) .0333(3) .0071(3) Cu1 .0152(4) .0182(4) .0143(4) -.0023(3) .0043(3) .0018(3) Cu2 .0220(3) .0230(3) .0197(3) -.0012(2) .0069(2) -.0038(2) O11 .0229(18) .0229(16) .0192(16) -.0026(13) .0106(14) .0027(13) C12 .035(3) .030(3) .024(2) -.002(2) .017(2) .005(2) C13 .041(3) .033(3) .020(2) .000(2) .017(2) .008(2) N14 .025(2) .032(2) .026(2) .0081(19) .0030(18) -.0046(19) C141 .044(3) .042(3) .032(3) .008(3) .023(3) .000(2) C142 .037(3) .046(3) .027(3) .009(3) .006(2) -.004(3) O21 .0243(17) .0147(15) .0226(16) -.0018(13) .0109(14) .0014(12) C22 .030(3) .020(2) .031(3) -.003(2) .016(2) .002(2) C23 .029(3) .020(2) .039(3) -.008(2) .017(2) .000(2) N24 .026(2) .035(2) .032(2) -.005(2) .009(2) -.008(2) C241 .047(4) .026(3) .052(4) -.009(3) .024(3) -.011(3) C242 .036(3) .052(4) .041(3) -.017(3) .005(3) -.011(3) O1 .027(2) .031(2) .039(2) .0035(16) .0107(17) .0038(17) S1 .0226(8) .0348(8) .0256(9) -.0042(6) .0112(6) -.0009(6) S1' .036(7) .036(7) .031(8) .007(5) .010(5) .003(5) C101 .039(3) .043(3) .040(3) -.009(3) .017(3) -.011(3) C102 .026(3) .036(3) .069(4) .005(2) .015(3) -.006(3) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published Cd1 Br1 . . 2.5733(6) ? Cd1 Br2 . . 2.6056(6) ? Cd1 Br3 . . 2.5821(9) ? Cd1 O21 . . 2.504(4) ? Cd1 O1 . . 2.374(4) ? Br1 Cu1 . . 3.0688(6) ? Br2 Cu2 . . 2.8300(9) ? Cu1 O11 . . 1.918(3) ? Cu1 O21 . . 1.997(3) ? Cu1 O11 . '7 566' 1.918(3) ? Cu1 O21 . '7 566' 1.997(3) ? Cu2 O11 . . 1.913(3) ? Cu2 N14 . . 2.091(5) ? Cu2 O21 . . 1.980(3) ? Cu2 N24 . . 2.069(4) ? O11 C12 . . 1.412(8) ? C12 C13 . . 1.516(6) ? C12 H12a . . .952 ? C12 H12b . . .955 ? C13 N14 . . 1.489(7) ? C13 H13a . . .959 ? C13 H13b . . .954 ? N14 C141 . . 1.477(9) ? N14 C142 . . 1.486(6) ? C141 H141a . . .944 ? C141 H141b . . .959 ? C141 H141c . . .950 ? C142 H142a . . .971 ? C142 H142b . . .962 ? C142 H142c . . .935 ? O21 C22 . . 1.432(6) ? C22 C23 . . 1.503(6) ? C22 H22a . . .947 ? C22 H22b . . .967 ? C23 N24 . . 1.495(9) ? C23 H23a . . .949 ? C23 H23b . . .981 ? N24 C241 . . 1.489(8) ? N24 C242 . . 1.475(6) ? C241 H241a . . .962 ? C241 H241b . . .949 ? C241 H241c . . .938 ? C242 H242a . . .958 ? C242 H242b . . .958 ? C242 H242c . . .958 ? O1 S1 . . 1.485(5) ? O1 S1' . . 1.517(12) ? S1 C101 . . 1.781(5) ? S1 C102 . . 1.775(6) ? S1' C101 . . 1.579(14) ? S1' C102 . . 1.648(16) ? C101 H101a . . .948 ? C101 H101b . . .957 ? C101 H101c . . .964 ? C101 H101'a . . .951 ? C101 H101'b . . .963 ? C101 H101'c . . .957 ? C102 H102a . . .983 ? C102 H102b . . .938 ? C102 H102c . . .958 ? C102 H102'a . . .917 ? C102 H102'b . . .978 ? C102 H102'c . . .963 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag #<< enter YES for value to be published Br1 Cd1 Br2 . . . 125.03(3) ? Br1 Cd1 Br3 . . . 114.68(2) ? Br1 Cd1 O21 . . . 87.53(7) ? Br1 Cd1 O1 . . . 92.17(8) ? Br2 Cd1 Br3 . . . 120.29(2) ? Br2 Cd1 O21 . . . 84.41(7) ? Br2 Cd1 O1 . . . 86.61(9) ? Br3 Cd1 O21 . . . 98.89(9) ? Br3 Cd1 O1 . . . 91.40(11) ? O21 Cd1 O1 . . . 168.80(14) ? Cd1 Br1 Cu1 . . . 79.306(16) ? Cd1 Br2 Cu2 . . . 80.41(2) ? Br1 Cu1 O11 . . . 87.88(11) ? Br1 Cu1 O21 . . . 85.00(10) ? Br1 Cu1 Br1 . . '7 566' 180.0000 ? Br1 Cu1 O11 . . '7 566' 92.12(11) ? Br1 Cu1 O21 . . '7 566' 95.00(10) ? O11 Cu1 O21 . . . 77.81(14) ? O11 Cu1 Br1 . . '7 566' 92.12(11) ? O11 Cu1 O11 . . '7 566' 180.0000 ? O11 Cu1 O21 . . '7 566' 102.19(14) ? O21 Cu1 Br1 . . '7 566' 95.00(10) ? O21 Cu1 O11 . . '7 566' 102.19(14) ? O21 Cu1 O21 . . '7 566' 180.0000 ? Br1 Cu1 O11 '7 566' . '7 566' 87.88(11) ? Br1 Cu1 O21 '7 566' . '7 566' 85.00(10) ? O11 Cu1 O21 '7 566' . '7 566' 77.81(14) ? Br2 Cu2 O11 . . . 97.01(11) ? Br2 Cu2 N14 . . . 96.96(12) ? Br2 Cu2 O21 . . . 89.28(10) ? Br2 Cu2 N24 . . . 96.35(14) ? O11 Cu2 N14 . . . 84.76(16) ? O11 Cu2 O21 . . . 78.35(14) ? O11 Cu2 N24 . . . 159.62(13) ? N14 Cu2 O21 . . . 162.60(15) ? N14 Cu2 N24 . . . 108.79(18) ? O21 Cu2 N24 . . . 86.51(16) ? Cu1 O11 Cu2 . . . 98.31(15) ? Cu1 O11 C12 . . . 131.2(3) ? Cu2 O11 C12 . . . 114.9(3) ? O11 C12 C13 . . . 106.6(5) ? O11 C12 H12a . . . 110.1 ? O11 C12 H12b . . . 110.1 ? C13 C12 H12a . . . 110.9 ? C13 C12 H12b . . . 110.4 ? H12a C12 H12b . . . 108.8 ? C12 C13 N14 . . . 109.7(4) ? C12 C13 H13a . . . 109.8 ? C12 C13 H13b . . . 110.5 ? N14 C13 H13a . . . 109.4 ? N14 C13 H13b . . . 109.1 ? H13a C13 H13b . . . 108.3 ? Cu2 N14 C13 . . . 101.7(3) ? Cu2 N14 C141 . . . 111.7(3) ? Cu2 N14 C142 . . . 117.2(4) ? C13 N14 C141 . . . 109.9(5) ? C13 N14 C142 . . . 107.9(4) ? C141 N14 C142 . . . 108.1(4) ? N14 C141 H141a . . . 109.9 ? N14 C141 H141b . . . 109.0 ? N14 C141 H141c . . . 110.1 ? H141a C141 H141b . . . 109.2 ? H141a C141 H141c . . . 109.9 ? H141b C141 H141c . . . 108.7 ? N14 C142 H142a . . . 109.7 ? N14 C142 H142b . . . 110.3 ? N14 C142 H142c . . . 111.6 ? H142a C142 H142b . . . 106.7 ? H142a C142 H142c . . . 108.8 ? H142b C142 H142c . . . 109.6 ? Cd1 O21 Cu1 . . . 106.57(12) ? Cd1 O21 Cu2 . . . 102.53(11) ? Cd1 O21 C22 . . . 116.6(3) ? Cu1 O21 Cu2 . . . 93.58(17) ? Cu1 O21 C22 . . . 123.7(3) ? Cu2 O21 C22 . . . 109.5(3) ? O21 C22 C23 . . . 107.6(4) ? O21 C22 H22a . . . 111.5 ? O21 C22 H22b . . . 110.6 ? C23 C22 H22a . . . 109.2 ? C23 C22 H22b . . . 109.8 ? H22a C22 H22b . . . 108.1 ? C22 C23 N24 . . . 110.9(5) ? C22 C23 H23a . . . 111.6 ? C22 C23 H23b . . . 109.1 ? N24 C23 H23a . . . 110.2 ? N24 C23 H23b . . . 108.0 ? H23a C23 H23b . . . 106.9 ? Cu2 N24 C23 . . . 102.4(3) ? Cu2 N24 C241 . . . 112.1(4) ? Cu2 N24 C242 . . . 117.2(3) ? C23 N24 C241 . . . 108.0(4) ? C23 N24 C242 . . . 108.5(5) ? C241 N24 C242 . . . 108.1(4) ? N24 C241 H241a . . . 109.2 ? N24 C241 H241b . . . 109.3 ? N24 C241 H241c . . . 110.0 ? H241a C241 H241b . . . 108.5 ? H241a C241 H241c . . . 109.3 ? H241b C241 H241c . . . 110.5 ? N24 C242 H242a . . . 110.8 ? N24 C242 H242b . . . 110.9 ? N24 C242 H242c . . . 110.9 ? H242a C242 H242b . . . 108.1 ? H242a C242 H242c . . . 108.0 ? H242b C242 H242c . . . 108.1 ? Cd1 O1 S1 . . . 132.6(2) ? Cd1 O1 S1' . . . 133.8(5) ? O1 S1 C101 . . . 108.2(3) ? O1 S1 C102 . . . 105.9(3) ? C101 S1 C102 . . . 98.2(3) ? O1 S1' C101 . . . 117.8(8) ? O1 S1' C102 . . . 110.9(7) ? C101 S1' C102 . . . 112.7(10) ? S1 C101 H101a . . . 111.1 ? S1 C101 H101b . . . 110.6 ? S1 C101 H101c . . . 110.1 ? S1' C101 H101'a . . . 109.9 ? S1' C101 H101'b . . . 111.5 ? S1' C101 H101'c . . . 110.7 ? H101a C101 H101b . . . 108.9 ? H101a C101 H101c . . . 108.4 ? H101b C101 H101c . . . 107.6 ? H101'a C101 H101'b . . . 108.2 ? H101'a C101 H101'c . . . 108.7 ? H101'b C101 H101'c . . . 107.7 ? S1 C102 H102a . . . 109.7 ? S1 C102 H102b . . . 112.3 ? S1 C102 H102c . . . 111.1 ? S1' C102 H102'a . . . 111.2(7) ? S1' C102 H102'b . . . 108.5(6) ? S1' C102 H102'c . . . 110.0(8) ? H102a C102 H102b . . . 107.7(7) ? H102a C102 H102c . . . 106.0(5) ? H102b C102 H102c . . . 109.7(7) ? H102'a C102 H102'b . . . 109.9(8) ? H102'a C102 H102'c . . . 111.1(6) ? H102'b C102 H102'c . . . 106.0(6) ? _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_analytical ? _chemical_formula_structural ? _exptl_crystal_F_000 2692 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 42 _reflns_limit_k_min 0 _reflns_limit_k_max 10 _reflns_limit_l_min -25 _reflns_limit_l_max 22 _reflns_number_observed ? _reflns_d_resolution_high .733 _reflns_d_resolution_low 13.808 _diffrn_reflns_av_sigmaI/netI .081 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 150 _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .058 _refine_ls_wR_factor_all .04 _refine_ls_goodness_of_fit_all 1.00 _refine_ls_shift/su_mean .0002 ####END #======================================================================= # Data block for single structure (one for each study in the paper) #======================================================================= data_lv612 _database_code_CSD 178074 # 2. EXPERIMENTAL DATA #--------------------- _chemical_formula_sum 'C24 H64 Cd4 Cl6 Cu2 N6 O8' _chemical_formula_moiety ? _chemical_formula_weight 1354.26 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P_1_21/n_1 _symmetry_space_group_name_Hall -p_2yn loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 8.835(2) _cell_length_b 11.865(2) _cell_length_c 21.463(4) _cell_angle_alpha 90.00000 _cell_angle_beta 91.105(5) _cell_angle_gamma 90.00000 _cell_volume 2249.5(8) _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.999 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 6012 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 20.4 _cell_measurement_temperature 150 _exptl_absorpt_coefficient_mu 3.187 _exptl_crystal_description prism _exptl_crystal_size_max .15 _exptl_crystal_size_mid .13 _exptl_crystal_size_min .08 _exptl_crystal_size_rad ? _exptl_crystal_colour blue _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .46 _exptl_absorpt_correction_T_max .69 _diffrn_reflns_number 42980 _reflns_number_total 11309 _reflns_Friedel_coverage 0 _reflns_number_gt 8499 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 37.32 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents 0.052 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 36 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .046 _refine_ls_wR_factor_ref .054 _refine_ls_goodness_of_fit_ref 1.563 _refine_ls_number_reflns 8499 _refine_ls_number_parameters 226 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .003 _refine_diff_density_min -2.21 _refine_diff_density_max 2.20 _refine_ls_extinction_method ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF SORTRF' _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 48 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 128 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' Cd ? 0 8 -1.005 1.202 'Int Tables Vol IV Tables 2.2B and 2.3.1' Cl ? 0 12 .132 .159 'Int Tables Vol IV Tables 2.2B and 2.3.1' Cu ? 0 4 .263 1.266 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 12 .004 .003 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 16 .008 .006 'Int Tables Vol IV Tables 2.2B and 2.3.1' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Cd1 .57309(3) .50943(2) .074343(10) .01593(10) Uani ? ? 1.00000 ? ? Cd2 .58456(3) .23344(2) .032156(12) .02161(12) Uani ? ? 1.00000 ? ? Cu1 .53751(5) .31135(4) .16982(2) .01877(19) Uani ? ? 1.00000 ? ? Cl1 .45492(10) .53524(7) .18145(4) .0223(4) Uani ? ? 1.00000 ? ? Cl2 .79932(10) .63591(8) .07772(4) .0268(4) Uani ? ? 1.00000 ? ? Cl3 .62777(12) .06526(9) .10153(5) .0328(5) Uani ? ? 1.00000 ? ? O11 .4202(3) .3201(2) .09270(13) .0245(12) Uani ? ? 1.00000 ? ? C12 .2681(5) .2867(4) .1034(2) .036(2) Uani ? ? 1.00000 ? ? C13 .2663(5) .1958(4) .1503(3) .039(2) Uani ? ? 1.00000 ? ? N14 .3544(4) .2308(3) .20724(18) .0311(17) Uani ? ? 1.00000 ? ? C141 .2624(6) .3044(4) .2470(2) .040(2) Uani ? ? 1.00000 ? ? C142 .3938(6) .1289(4) .2444(3) .048(3) Uani ? ? 1.00000 ? ? O21 .7000(3) .3523(2) .11424(11) .0199(11) Uani ? ? 1.00000 ? ? C22 .8410(4) .3597(4) .1450(2) .0298(19) Uani ? ? 1.00000 ? ? C23 .8103(5) .3954(3) .2123(2) .033(2) Uani ? ? 1.00000 ? ? N24 .6976(4) .3204(3) .23980(15) .0270(15) Uani ? ? 1.00000 ? ? C241 .6484(6) .3707(4) .2991(2) .041(2) Uani ? ? 1.00000 ? ? C242 .7705(6) .2086(4) .2529(2) .036(2) Uani ? ? 1.00000 ? ? O31 .6073(3) .4055(2) -.01576(10) .0163(10) Uani ? ? 1.00000 ? ? C32 .7549(4) .4057(3) -.04121(16) .0206(15) Uani ? ? 1.00000 ? ? C33 .7862(4) .2970(3) -.07480(16) .0236(16) Uani ? ? 1.00000 ? ? N34 .7814(4) .1984(3) -.03252(15) .0240(14) Uani ? ? 1.00000 ? ? C341 .7595(5) .0931(4) -.0683(2) .037(2) Uani ? ? 1.00000 ? ? C342 .9231(5) .1890(4) .0048(2) .037(2) Uani ? ? 1.00000 ? ? O01 .3913(4) .1622(3) -.02880(18) .049(2) Uani ? ? 1.00000 ? ? H12a .21240 .35005 .11837 .04500 Uiso ? ? 1.00000 ? ? H12b .22242 .26088 .06575 .04500 Uiso ? ? 1.00000 ? ? H13a .31084 .12961 .13394 .04900 Uiso ? ? 1.00000 ? ? H13b .16503 .17994 .16192 .04900 Uiso ? ? 1.00000 ? ? H141a .31993 .32668 .28268 .05900 Uiso ? ? 1.00000 ? ? H141b .17424 .26549 .25950 .05900 Uiso ? ? 1.00000 ? ? H141c .23288 .37016 .22400 .05900 Uiso ? ? 1.00000 ? ? H142a .45009 .15108 .28083 .07100 Uiso ? ? 1.00000 ? ? H142b .45311 .07955 .22036 .07100 Uiso ? ? 1.00000 ? ? H142c .30380 .09195 .25661 .07100 Uiso ? ? 1.00000 ? ? H22a .90222 .41476 .12547 .03600 Uiso ? ? 1.00000 ? ? H22b .89064 .28905 .14465 .03600 Uiso ? ? 1.00000 ? ? H23a .77452 .47058 .21252 .04100 Uiso ? ? 1.00000 ? ? H23b .90267 .39091 .23595 .04100 Uiso ? ? 1.00000 ? ? H241a .57504 .32229 .31772 .06300 Uiso ? ? 1.00000 ? ? H241b .60530 .44216 .29192 .06300 Uiso ? ? 1.00000 ? ? H241c .73321 .37721 .32705 .06300 Uiso ? ? 1.00000 ? ? H242a .69902 .15938 .27092 .05400 Uiso ? ? 1.00000 ? ? H242b .85358 .21915 .28143 .05400 Uiso ? ? 1.00000 ? ? H242c .80629 .17728 .21540 .05400 Uiso ? ? 1.00000 ? ? H32a .82755 .41516 -.00848 .02600 Uiso ? ? 1.00000 ? ? H32b .76247 .46672 -.06978 .02600 Uiso ? ? 1.00000 ? ? H33a .88384 .30110 -.09263 .03000 Uiso ? ? 1.00000 ? ? H33b .71218 .28709 -.10716 .03000 Uiso ? ? 1.00000 ? ? H341a .75643 .03099 -.04087 .05500 Uiso ? ? 1.00000 ? ? H341b .84057 .08410 -.09644 .05500 Uiso ? ? 1.00000 ? ? H341c .66653 .09754 -.09160 .05500 Uiso ? ? 1.00000 ? ? H342a .91733 .12546 .03164 .05400 Uiso ? ? 1.00000 ? ? H342b .93690 .25531 .02913 .05400 Uiso ? ? 1.00000 ? ? H342c 1.00614 .18021 -.02218 .05400 Uiso ? ? 1.00000 ? ? H01a .34718 .20047 -.05538 .10000 Uiso ? ? 1.00000 ? ? H01b .39726 .09044 -.04627 .02600 Uiso ? ? 1.00000 ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Cd1 .01772(10) .01451(10) .01554(10) .00045(8) .00040(7) .00041(8) Cd2 .02235(12) .02112(12) .02144(12) .00125(9) .00265(9) -.00293(9) Cu1 .0215(2) .01778(19) .01711(18) -.00199(15) .00189(14) .00255(15) Cl1 .0273(4) .0207(4) .0192(3) .0019(3) .0039(3) -.0013(3) Cl2 .0230(4) .0241(4) .0331(4) -.0069(3) -.0008(3) .0012(3) Cl3 .0367(5) .0273(5) .0345(5) .0000(4) .0025(4) -.0057(4) O11 .0216(12) .0245(13) .0273(13) -.0040(10) -.0037(10) -.0010(10) C12 .0222(18) .038(2) .047(3) -.0077(16) -.0032(17) .000(2) C13 .029(2) .027(2) .062(3) -.0074(16) .016(2) -.004(2) N14 .0317(17) .0211(15) .041(2) -.0007(13) .0138(14) .0059(14) C141 .043(2) .030(2) .048(3) -.0006(19) .025(2) .0040(19) C142 .050(3) .028(2) .066(3) .002(2) .025(2) .021(2) O21 .0180(11) .0212(11) .0205(11) .0014(9) .0015(8) .0027(9) C22 .0195(16) .031(2) .039(2) .0000(14) -.0026(14) .0119(17) C23 .034(2) .0221(17) .041(2) -.0030(15) -.0193(17) -.0002(16) N24 .0402(19) .0184(14) .0220(14) .0036(13) -.0051(13) .0009(11) C241 .068(3) .036(2) .0205(18) .013(2) -.0097(19) -.0038(17) C242 .049(3) .0248(19) .034(2) .0087(18) -.0060(19) .0051(16) O31 .0156(10) .0177(10) .0157(10) .0010(8) .0027(8) -.0002(8) C32 .0183(14) .0221(16) .0216(15) -.0003(12) .0034(11) .0011(12) C33 .0225(16) .0271(17) .0214(15) .0028(13) .0077(12) -.0009(13) N34 .0218(14) .0225(14) .0279(15) .0009(11) .0038(11) .0020(12) C341 .042(2) .0240(19) .045(2) .0016(17) .016(2) -.0054(17) C342 .0230(18) .041(2) .046(3) .0032(17) .0006(17) .017(2) O01 .056(2) .0311(17) .059(2) .0091(15) -.0339(18) -.0173(15) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag #<< enter YES for value to be published Cd1 Cl1 . . 2.5614(10) ? Cd1 Cl2 . . 2.4993(10) ? Cd1 O11 . . 2.655(3) ? Cd1 O21 . . 2.330(2) ? Cd1 O31 . . 2.318(2) ? Cd1 O31 . '3 665' 2.250(2) ? Cd2 Cl3 . . 2.5145(11) ? Cd2 O11 . . 2.220(3) ? Cd2 O21 . . 2.462(2) ? Cd2 O31 . . 2.296(2) ? Cd2 N34 . . 2.284(3) ? Cd2 O01 . . 2.292(4) ? Cu1 Cl1 . . 2.7674(11) ? Cu1 O11 . . 1.939(3) ? Cu1 N14 . . 2.056(4) ? Cu1 O21 . . 1.945(2) ? Cu1 N24 . . 2.046(3) ? O11 C12 . . 1.424(5) ? C12 C13 . . 1.476(7) ? C12 H12a . . .957 ? C12 H12b . . .947 ? C13 N14 . . 1.494(6) ? C13 H13a . . .949 ? C13 H13b . . .952 ? N14 C141 . . 1.476(6) ? N14 C142 . . 1.485(6) ? C141 H141a . . .949 ? C141 H141b . . .948 ? C141 H141c . . .957 ? C142 H142a . . .956 ? C142 H142b . . .946 ? C142 H142c . . .949 ? O21 C22 . . 1.401(5) ? C22 C23 . . 1.534(6) ? C22 H22a . . .951 ? C22 H22b . . .947 ? C23 N24 . . 1.468(5) ? C23 H23a . . .947 ? C23 H23b . . .954 ? N24 C241 . . 1.479(6) ? N24 C242 . . 1.500(5) ? C241 H241a . . .959 ? C241 H241b . . .940 ? C241 H241c . . .954 ? C242 H242a . . .948 ? C242 H242b . . .955 ? C242 H242c . . .947 ? O31 C32 . . 1.423(4) ? C32 C33 . . 1.506(5) ? C32 H32a . . .949 ? C32 H32b . . .952 ? C33 N34 . . 1.482(5) ? C33 H33a . . .952 ? C33 H33b . . .952 ? N34 C341 . . 1.477(5) ? N34 C342 . . 1.478(5) ? C341 H341a . . .943 ? C341 H341b . . .952 ? C341 H341c . . .955 ? C342 H342a . . .950 ? C342 H342b . . .950 ? C342 H342c . . .950 ? O01 H01a . . .822 ? O01 H01b . . .933 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag #<< enter YES for value to be published Cl1 Cd1 Cl2 . . . 103.99(3) ? Cl1 Cd1 O11 . . . 75.56(6) ? Cl1 Cd1 O21 . . . 88.13(6) ? Cl1 Cd1 O31 . . . 150.95(6) ? Cl1 Cd1 O31 . . '3 665' 98.70(6) ? Cl2 Cd1 O11 . . . 155.89(6) ? Cl2 Cd1 O21 . . . 95.22(6) ? Cl2 Cd1 O31 . . . 103.09(6) ? Cl2 Cd1 O31 . . '3 665' 107.72(6) ? O11 Cd1 O21 . . . 60.72(8) ? O11 Cd1 O31 . . . 75.44(8) ? O11 Cd1 O31 . . '3 665' 96.05(8) ? O21 Cd1 O31 . . . 79.12(8) ? O21 Cd1 O31 . . '3 665' 153.49(8) ? O31 Cd1 O31 . . '3 665' 82.82(8) ? Cl3 Cd2 O11 . . . 96.58(7) ? Cl3 Cd2 O21 . . . 88.54(6) ? Cl3 Cd2 O31 . . . 163.14(6) ? Cl3 Cd2 N34 . . . 96.12(8) ? Cl3 Cd2 O01 . . . 98.53(9) ? O11 Cd2 O21 . . . 65.32(9) ? O11 Cd2 O31 . . . 85.08(9) ? O11 Cd2 N34 . . . 162.64(11) ? O11 Cd2 O01 . . . 90.94(12) ? O21 Cd2 O31 . . . 76.87(8) ? O21 Cd2 N34 . . . 103.26(10) ? O21 Cd2 O01 . . . 155.94(11) ? O31 Cd2 N34 . . . 79.36(10) ? O31 Cd2 O01 . . . 98.21(10) ? N34 Cd2 O01 . . . 98.83(12) ? Cl1 Cu1 O11 . . . 83.57(8) ? Cl1 Cu1 N14 . . . 101.56(10) ? Cl1 Cu1 O21 . . . 90.85(8) ? Cl1 Cu1 N24 . . . 93.61(9) ? O11 Cu1 N14 . . . 86.94(13) ? O11 Cu1 O21 . . . 81.48(11) ? O11 Cu1 N24 . . . 167.06(12) ? N14 Cu1 O21 . . . 161.99(13) ? N14 Cu1 N24 . . . 106.00(14) ? O21 Cu1 N24 . . . 85.95(12) ? Cd1 Cl1 Cu1 . . . 72.03(2) ? Cd1 O11 Cd2 . . . 87.97(9) ? Cd1 O11 Cu1 . . . 84.65(9) ? Cd1 O11 C12 . . . 138.1(2) ? Cd2 O11 Cu1 . . . 97.46(11) ? Cd2 O11 C12 . . . 126.6(3) ? Cu1 O11 C12 . . . 109.7(3) ? O11 C12 C13 . . . 109.6(3) ? O11 C12 H12a . . . 109.1 ? O11 C12 H12b . . . 109.9 ? C13 C12 H12a . . . 109.5 ? C13 C12 H12b . . . 109.6 ? H12a C12 H12b . . . 109.1 ? C12 C13 N14 . . . 110.0(4) ? C12 C13 H13a . . . 110.0 ? C12 C13 H13b . . . 110.1 ? N14 C13 H13a . . . 108.7 ? N14 C13 H13b . . . 108.6 ? H13a C13 H13b . . . 109.4 ? Cu1 N14 C13 . . . 102.2(3) ? Cu1 N14 C141 . . . 113.4(3) ? Cu1 N14 C142 . . . 114.2(3) ? C13 N14 C141 . . . 110.7(3) ? C13 N14 C142 . . . 109.0(3) ? C141 N14 C142 . . . 107.3(4) ? N14 C141 H141a . . . 109.9 ? N14 C141 H141b . . . 109.9 ? N14 C141 H141c . . . 109.4 ? H141a C141 H141b . . . 109.7 ? H141a C141 H141c . . . 109.0 ? H141b C141 H141c . . . 109.0 ? N14 C142 H142a . . . 109.2 ? N14 C142 H142b . . . 109.7 ? N14 C142 H142c . . . 109.6 ? H142a C142 H142b . . . 109.3 ? H142a C142 H142c . . . 109.1 ? H142b C142 H142c . . . 109.9 ? Cd1 O21 Cd2 . . . 90.32(8) ? Cd1 O21 Cu1 . . . 93.99(10) ? Cd1 O21 C22 . . . 122.6(2) ? Cd2 O21 Cu1 . . . 89.75(9) ? Cd2 O21 C22 . . . 136.5(2) ? Cu1 O21 C22 . . . 112.7(2) ? O21 C22 C23 . . . 106.8(3) ? O21 C22 H22a . . . 110.1 ? O21 C22 H22b . . . 110.4 ? C23 C22 H22a . . . 109.8 ? C23 C22 H22b . . . 110.0 ? H22a C22 H22b . . . 109.7 ? C22 C23 N24 . . . 110.2(3) ? C22 C23 H23a . . . 109.3 ? C22 C23 H23b . . . 108.7 ? N24 C23 H23a . . . 109.8 ? N24 C23 H23b . . . 109.4 ? H23a C23 H23b . . . 109.4 ? Cu1 N24 C23 . . . 101.6(2) ? Cu1 N24 C241 . . . 116.3(3) ? Cu1 N24 C242 . . . 112.3(3) ? C23 N24 C241 . . . 108.3(3) ? C23 N24 C242 . . . 108.6(3) ? C241 N24 C242 . . . 109.1(3) ? N24 C241 H241a . . . 109.2 ? N24 C241 H241b . . . 110.3 ? N24 C241 H241c . . . 109.4 ? H241a C241 H241b . . . 109.5 ? H241a C241 H241c . . . 108.4 ? H241b C241 H241c . . . 110.0 ? N24 C242 H242a . . . 109.5 ? N24 C242 H242b . . . 109.0 ? N24 C242 H242c . . . 109.7 ? H242a C242 H242b . . . 109.3 ? H242a C242 H242c . . . 110.0 ? H242b C242 H242c . . . 109.4 ? Cd1 O31 Cd2 . . . 94.90(8) ? Cd1 O31 C32 . . . 117.02(19) ? Cd1 O31 Cd1 . . '3 665' 97.18(9) ? Cd2 O31 C32 . . . 105.23(19) ? Cd2 O31 Cd1 . . '3 665' 125.58(10) ? C32 O31 Cd1 . . '3 665' 115.39(19) ? O31 C32 C33 . . . 111.1(3) ? O31 C32 H32a . . . 109.1 ? O31 C32 H32b . . . 109.0 ? C33 C32 H32a . . . 109.1 ? C33 C32 H32b . . . 109.1 ? H32a C32 H32b . . . 109.4 ? C32 C33 N34 . . . 112.1(3) ? C32 C33 H33a . . . 108.9 ? C32 C33 H33b . . . 109.0 ? N34 C33 H33a . . . 108.9 ? N34 C33 H33b . . . 108.8 ? H33a C33 H33b . . . 109.2 ? Cd2 N34 C33 . . . 105.0(2) ? Cd2 N34 C341 . . . 112.1(3) ? Cd2 N34 C342 . . . 109.3(3) ? C33 N34 C341 . . . 110.8(3) ? C33 N34 C342 . . . 111.0(3) ? C341 N34 C342 . . . 108.6(3) ? N34 C341 H341a . . . 110.0 ? N34 C341 H341b . . . 109.4 ? N34 C341 H341c . . . 109.1 ? H341a C341 H341b . . . 109.9 ? H341a C341 H341c . . . 109.6 ? H341b C341 H341c . . . 108.8 ? N34 C342 H342a . . . 109.5 ? N34 C342 H342b . . . 109.5 ? N34 C342 H342c . . . 109.4 ? H342a C342 H342b . . . 109.4 ? H342a C342 H342c . . . 109.5 ? H342b C342 H342c . . . 109.5 ? Cd2 O01 H01a . . . 122.1 ? Cd2 O01 H01b . . . 121.3 ? H01a O01 H01b . . . 104.8 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag #<< enter YES for value to be published ? ? ? ? ? ? ? ? ? ? ? #-------------------------------------------------------------------------- # Special items requested by author for inclusion in paper #-------------------------------------------------------------------------- loop_ _publ_manuscript_incl_extra_item _publ_manuscript_incl_extra_defn ? ? #-------------------------------------------------------------------------- # Items which are non-mandatory for Acta C submissions #-------------------------------------------------------------------------- _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _geom_special_details ? _cell_special_details ; ? ; _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_analytical ? _chemical_formula_structural ? _exptl_crystal_F_000 1332 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 15 _reflns_limit_k_min 0 _reflns_limit_k_max 19 _reflns_limit_l_min -36 _reflns_limit_l_max 36 _reflns_number_observed ? _reflns_d_resolution_high .586 _reflns_d_resolution_low 8.211 _diffrn_reflns_av_sigmaI/netI .073 _diffrn_reflns_theta_min 2.48 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 150 _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .07 _refine_ls_wR_factor_all .058 _refine_ls_goodness_of_fit_all 1.434 _refine_ls_shift/su_mean .0001 #END